CN109873080B - Perovskite single crystal X-ray detector and preparation method thereof - Google Patents
Perovskite single crystal X-ray detector and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a perovskite single crystal X-ray detector and a preparation method thereof, the perovskite single crystal X-ray detector comprises a perovskite single crystal and electrodes on the upper side and the lower side of the single crystal, and the perovskite single crystal is (NH) 2 CH＝NH 2 )PbI 3 The molecular formula of the perovskite single crystal growth solution is (NH) prepared by adding rubidium halide and lead halide 2 CH＝NH 2 ) x Rb 1‑x Pb(I y Br 1‑y ) 3 Wherein 0.9 ≦ x < 1,0.8 ≦ y < 1. The rubidium halide and lead halide doped material can inhibit (NH) 2 CH＝NH 2 )PbI 3 The phase change from black phase to yellow phase of the single crystal can effectively improve the ion migration in the single crystal, and the performance of the single crystal is effectively improved.
Description
Technical Field
The invention belongs to the field of perovskite single crystal X-ray detectors, and particularly relates to a perovskite single crystal X-ray detector and a preparation method thereof.
Background
In recent years, photodetectors capable of converting incident light (ultraviolet, visible or infrared) into electrical signals have become important for various industrial and scientific applications including imaging, optical communication, environmental monitoring and biosensing. (NH) 2 CH＝NH 2 )PbI 3 Is an organic-inorganic hybrid perovskite single crystal with a typical formula, and has long electric property due to the direct band gapThe long transport lengths of the electrons and holes and the high absorption coefficients have attracted extensive research interest. These unique characteristics give perovskites unique electrical and optoelectronic characteristics. Perovskites have large optical absorption coefficients over a wide wavelength range of 300-800nm, which is ideal for broadband photodetector applications. Furthermore, due to its high absorption capacity and direct bandgap properties, complete light absorption can be achieved by very thin perovskite layers (several hundred nm). The small moving distance of the photo-generated charge carriers results in a fast photo-response speed. These properties strongly suggest that organic-inorganic hybrid perovskite materials are ideal building blocks for high performance photodetectors.
Disclosure of Invention
Due to (NH) 2 CH＝NH 2 )PbI 3 At normal temperature, under the conditions of moisture and oxygen, the single crystal is easy to change from black phase to yellow phase, and (NH) is seriously influenced 2 CH＝NH 2 )PbI 3 The single crystal's test performance against light may be considered to be suppressed by doping it with certain metal cations. Meanwhile, the added metal ions can also improve the performance of the single crystal.
Recently, optical and electrical studies have shown that single crystal perovskites exhibit enhanced properties in terms of trap density and charge transport characteristics compared to their polycrystalline thin film counterparts. For example, no significant absorption peak near the band gap of the single crystal was observed, indicating its more ordered structure. Single crystals have low defect state density and longer carrier diffusion length. Furthermore, it has a longer charge carrier lifetime compared to polycrystalline thin films, due to lower defect state-induced recombination. The diffusion length of single crystals is reported to far exceed the measured value for polycrystalline films. All of these results may indicate that optoelectronic devices made from single crystal perovskites may exhibit better performance than polycrystalline counterparts. As described above, in order to improve the performance of a perovskite-based X-ray detector, one possible approach is to reduce the grain boundaries and defect density to reduce the recombination of photogenerated carriers and increase the carrier lifetime. Therefore, an X-ray detector composed of single crystal perovskites can achieve the desired photoconductive properties.
The invention aims to overcome the defects of the prior art and provides a perovskite single crystal X-ray detector and a preparation method thereof 2 CH＝NH 2 )PbI 3 Rubidium halide and lead halide are doped to improve the performance of the X-ray detector.
One of the purposes of the invention is realized by the following technical scheme:
a perovskite single crystal X-ray detector comprises a perovskite single crystal and electrodes on the upper side and the lower side of the single crystal, wherein the perovskite single crystal is (NH) 2 CH＝NH 2 )PbI 3 Rubidium halide and lead halide are added into the solution for growing the perovskite monocrystal to prepare the (NH) molecular formula 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 Wherein 0.9 ≦ x < 1,0.8 ≦ y < 1.
Further, the electrode material is gold.
Further, the electrodes were made using a square electrode template with a gold plating layer thickness of 100nm.
Further, the rubidium halide is rubidium iodide or rubidium bromide.
Further, the lead halide is lead iodide or lead bromide.
The other purpose of the invention is realized by the following technical scheme:
a preparation method of a perovskite single crystal X-ray detector comprises the following steps:
(1) Preparation of perovskite Single Crystal
Mixing (NH) with the molar ratio of (0.9-1) to (0.8-1) 2 CH＝NH 2 ) I and PbI 2 Mixed and dissolved in gamma-butyrolactone to form (NH) 2 CH＝NH 2 )PbI 3 Adding rubidium halide and lead halide, mixing and stirring until the materials are completely dissolved to form (NH) 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 Heating the solution at 120-125 deg.C until small 1mm black crystals are formed, removingSmall black crystal particles; transferring the generated black particles into New (NH) 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 Continuously growing to 1cm in the solution to prepare perovskite single crystal; said New (NH) 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 The solution is prepared by mixing the following components in a molar ratio of (0.9-1): (0.8-1) of (NH) 2 CH＝NH 2 ) I and PbI 2 Mixing and dissolving the mixture into gamma-butyrolactone, and adding rubidium halide and lead halide into the mixture to obtain the product;
(2) X-ray detector for preparing perovskite single crystal
Cleaning the perovskite single crystal generated in the step (1) with ethanol, selecting the upper and lower smooth surfaces, and evaporating gold electrodes on two sides of the single crystal by using a square electrode template.
Further, said added (NH) 2 CH＝NH 2 ) I, rubidium halide, pbI 2 The molar ratio of the lead halide to the lead halide is (0.9-1) to (0-0.1) to (0.8-1) to (0-0.2).
Further, said added (NH) 2 CH＝NH 2 ) I, rubidium halide, pbI 2 And lead halide in a molar ratio of 0.95.
Further, said added (NH) 2 CH＝NH 2 ) I, rubidium halide, pbI 2 And the molar ratio of lead halide is 0.9.
Further, said added (NH) 2 CH＝NH 2 ) I, rubidium halide, pbI 2 And a molar ratio of lead halide of 0.95.
Compared with the prior art, the invention has the following advantages:
(1)(NH 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 single crystals have a large optical absorption coefficient, high carrier mobility, long carrier lifetime and long diffusion length.
(2) The doped iodide material of the invention can inhibit (NH) 2 CH＝NH 2 )PbI 3 Phase transition of single crystal from black phase to yellow phaseMeanwhile, the ion migration in the single crystal can be effectively improved, so that the performance of the single crystal is effectively improved.
(3) The invention effectively reduces the defect state density of the single crystal by ion doping.
(4) The invention improves the responsivity of the single crystal X-ray detector by ion doping.
(5) The invention effectively widens the response frequency of the X-ray detector through ion doping.
Drawings
FIG. 1 is a structural diagram of a perovskite single crystal X-ray detector, wherein 1 is an electrode, and 2 is a perovskite single crystal.
FIG. 2 is (NH) 2 CH＝NH 2 )PbI 3 Photocurrent test chart of perovskite single crystal X-ray detector doped with rubidium ions with different amounts and lead bromide with different amounts, wherein the single crystal in comparative example 1 is in molar ratio (NH) 2 CH＝NH 2 )I：PbI 2 A perovskite single crystal grown from a material of = 1:1; the single crystal of example 1 was in a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 0.95, 0.05; the single crystal of example 2 was in a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 A perovskite single crystal grown from a material of = 0.9.1; the single crystal of example 3 was in a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 0.95, 0.05; the single crystal of example 4 was at a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 0.9.
FIG. 3 is (NH) 2 CH＝NH 2 )PbI 3 Sensitivity test chart of X-ray detector doped with rubidium ions and lead bromide in different amounts for perovskite single crystal X-ray detector, wherein single crystal in comparative example 1 is in molar ratio (NH) 2 CH＝NH 2 )I：PbI 2 A perovskite single crystal grown from a material of = 1:1; the single crystal of example 1 was in a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 ＝0.95:0.05:0.9:01 perovskite single crystal grown from the material of; the single crystal of example 2 was in a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 A perovskite single crystal grown from a material of = 0.9.1; the single crystal of example 3 was in a molar ratio (NH) 2 CH＝NH 2 ) I: rbI: pbI2, pbBr2= 0.95; the single crystal of example 4 was at a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 0.9.
FIG. 4 shows (NH) 2 CH＝NH 2 )PbI 3 Response test chart of X-ray detector doped with different amounts of rubidium ions and lead bromide of perovskite single crystal X-ray detector, wherein the single crystal in comparative example 1 is in molar ratio (NH) 2 CH＝NH 2 )I：PbI 2 A perovskite single crystal grown from a material of = 1:1; the single crystal of example 1 was in a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 0.95, 0.05; the single crystal of example 2 was in a molar ratio (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 A perovskite single crystal grown from a material of = 0.9.1; the single crystal of example 3 was in a molar ratio (NH) 2 CH＝NH 2 ) I: rbI: pbI2 PbBr2= 0.95.
Detailed Description
To further illustrate the technical means and effects of the present invention, the following further describes the technical solution of the present invention with reference to the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.
Comparative example 1 preparation (NH) 2 CH＝NH 2 )PbI 3 Perovskite single crystal X-ray detector
1) Preparation of (NH) 2 CH＝NH 2 )PbI 3 Perovskite single crystal
The method comprises the following specific steps: 172mg of (NH) 2 CH＝NH 2 ) I and 461mg of PbI 2 Mixed and dissolved in 1mL of gamma-butyrolactone to form HC (NH) 2 ) 2 PbI 3 And mixing and stirring the solution until the solution is clear and completely dissolved. Transferring the solution into a heatable flat-bottomed flask, placing on a heating table with an initial temperature of 120-125 deg.C, heating, and transferring 1 of the solution to new 2mL (NH) when black crystal particles with a diameter of about 1mm appear at the bottom of the flask 2 CH＝NH 2 )PbI 3 Continuously growing to 1cm in the solution; said New (NH) 2 CH＝NH 2 )PbI 3 The solution is passed through a reactor at a molar ratio of 1:1 (NH) 2 CH＝NH 2 ) I and PbI 2 Mixing and dissolving the mixture into gamma-butyrolactone to obtain the product.
2)(NH 2 CH＝NH 2 )PbI 3 Preparation of perovskite single crystal X-ray detector
Cleaning the grown single crystal with ethanol, selecting two smooth upper and lower surfaces, and respectively evaporating a layer of gold electrode with the thickness of 100nm on the upper and lower surfaces of the single crystal by using a square electrode template. The test is then performed.
3)(NH 2 CH＝NH 2 )PbI 3 Testing of perovskite single crystal X-ray detectors
(NH 2 CH＝NH 2 )PbI 3 After the perovskite single crystal X-ray detector is manufactured, a series of tests related to the performance of the detector are carried out on the perovskite single crystal X-ray detector. One is a current change test at different X-ray radiation doses. The second is sensitivity testing at different bias voltages. And thirdly, response test. Specifically, the first test was conducted at 5.5mGyairs -1 The photocurrent of the detector was 3.98uA cm -2 . The second test, at 150V bias, the sensitivity of the detector was 1358uC Gy-1air cm -2 . In the third test, the difference in the dark current of the detector was 16.5nA.
Example 1 preparation of (NH) 2 CH＝NH 2 ) 0.95 Rb 0.05 Pb(I 0.9 Br 0.1 ) 3 Perovskite crystal detector
1) Preparation of (NH) 2 CH＝NH 2 ) 0.95 Rb 0.05 Pb(I 0.9 Br 0.1 ) 3 Perovskite single crystal
The method comprises the following specific steps: 163mg of (NH) 2 CH＝NH 2 ) I and 414.9mg of PbI 2 Mixed and dissolved in 1mL of gamma-butyrolactone to form (NH) 2 CH＝NH 2 )PbI 3 Solution, then adding RbI to (NH) above 2 CH＝NH 2 )PbI 3 Adding PbBr into the solution until the RbI mass concentration is 10.65mg/ml 2 To the above (NH) 2 CH＝NH 2 )PbI 3 Solution to PbBr 2 The mixture with the mass concentration of 36.7mg/ml is stirred until the solution is clear. Transferring the solution into a heatable flat-bottomed bottle, placing the bottle on a heating table with the initial temperature of 120-125 ℃, heating, and transferring 1 of the solution into a new same solution to continue to grow to 1cm when black crystal particles with the diameter of about 1mm appear at the bottom of the bottle; said New (NH) 2 CH＝NH 2 ) 0.95 Rb 0.05 Pb(I 0.9 Br 0.1 ) 3 The solution is (NH) 2 CH＝NH 2 )I：RbI：PbI 2 :PbBr 2 The molar ratio of 0.95.
2)(NH 2 CH＝NH 2 ) 0.95 Rb 0.05 Pb(I 0.9 Br 0.1 ) 3 Preparation of perovskite single crystal X-ray detector
Cleaning the grown single crystal with ethanol, selecting two smooth upper and lower surfaces, and respectively evaporating a layer of gold electrode with the thickness of 100nm on the upper and lower surfaces of the single crystal by using a square electrode template. The test is then performed.
3)(NH 2 CH＝NH 2 ) 0.95 Rb 0.05 Pb(I 0.9 Br 0.1 ) 3 Testing of perovskite single crystal X-ray detectors
(NH 2 CH＝NH 2 ) 0.95 Rb 0.05 Pb(I 0.9 Br 0.1 ) 3 After the perovskite single crystal X-ray detector is manufactured, a series of tests related to the performance of the detector are carried out on the perovskite single crystal X-ray detector. One is a current change test at different X-ray radiation doses. The second is sensitivity testing at different bias voltages. Third, response test to light in dark state. Specifically, the first test was conducted at 5.5mGyairs -1 In the following, the first and second parts of the material,the photocurrent of the detector was 6.01uA cm -2 . The second test, under 150V bias, the sensitivity of the detector is 1511uC Gy-1air cm -2 . In the third test, the difference in the dark current of the detector was 20.1nA.
Example 2 preparation of (NH) 2 CH＝NH 2 ) 0.9 Rb 0.1 Pb(I 0.9 Br 0.1 ) 3 Perovskite crystal detector
The procedure of example 1 was followed to increase the concentration of RbI until the RbI mass concentration was 21.3mg/mL. PbBr 2 The concentration of (c) is kept constant.
First, at 5.5mGyairs -1 The photocurrent of the detector is 11.048uA cm -2 . The second test, at 150V bias, has a probe sensitivity of 2600uC Gy-1air cm -2 . In the third test, the difference in the dark current of the detector was 22.5nA.
Example 3 preparation of (NH) 2 CH＝NH 2 ) 0.95 Rb 0.05 Pb(I 0.8 Br 0.2 ) 3 Perovskite crystal detector
PbBr was increased according to the procedure of example 1 2 To PbBr concentration 2 The mass concentration was 73.4mg/mL. The concentration of RbI remained unchanged.
The first test, at 5.5mGyairs -1 The photocurrent of the detector was 12.91uA cm -2 . The second test, under 150V bias, the sensitivity of the detector is 3508uC Gy-1air cm -2 . In the third test, the detector has a light dark current difference of 25nA.
Example 4 preparation of (NH) 2 CH＝NH 2 ) 0.9 Rb 0.1 Pb(I 0.8 Br 0.2 ) 3 Perovskite crystal detector
Following the procedure of example 1, the RbI concentration was increased until the RbI mass concentration was 21.3mg/mL, and PbBr was increased 2 To PbBr concentration 2 The mass concentration was 73.4mg/mL.
The first test, at 5.5mGyairs -1 At this time, the photocurrent of the detector was 15.14uA cm -2 . The second test, at 150V bias,the sensitivity of the detector is 4500uC Gy-1air cm -2 . In the third test, the difference in the dark current of the detector was 26.5nA.
(NH) of different doping amounts of rubidium ions and lead bromide in Table 1, comparative example 1, and examples 1 to 4 2 CH＝NH 2 )PbI 3 Performance of perovskite single crystal X-ray detector.
| Photocurrent (uA cm) -2 ) | Sensitivity (uCGy) -1 air cm -2 ) | Current (nA) | |
| Comparative example 1 | 3.98 | 1358 | 16.5 |
| Example 1 | 6.01 | 1511 | 20.1 |
| Example 2 | 11.48 | 2600 | 22.5 |
| Example 3 | 12.91 | 3508 | 25.4 |
| Example 4 | 15.14 | 4500 | 26.5 |
From the above, in pure (NH) 2 CH＝NH 2 )PbI 3 Rubidium ions and lead bromide are doped into the single crystal, and the phase change of the single crystal is inhibited to a certain extent. The performance of the detector is improved to a certain extent when the detector is tested.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent alterations and modifications are intended to be included within the scope of the present invention, without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a perovskite single crystal X-ray detector is characterized by comprising the following steps:
(1) Preparation of perovskite Single Crystal
Mixing (NH) with the molar ratio of (0.9-1) to (0.8-1) 2 CH＝NH 2 ) I and PbI 2 Mixed and dissolved in gamma-butyrolactone to form (NH) 2 CH＝NH 2 )PbI 3 Adding rubidium halide and lead halide, mixing and stirring until the materials are completely dissolved to form (NH) 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 Heating the solution at 120-125 deg.C until 1mm black crystal granule is formed, and removing the black crystal granule; transferring the generated black particles into New (NH) 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 Continuously growing to 1cm in the solution to prepare perovskite single crystal; said New (NH) 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 The solution is prepared by mixing the following components in a molar ratio of (0.9-1): (0.8-1) of (NH) 2 CH＝NH 2 ) I and PbI 2 Mixing and dissolving the mixture into gamma-butyrolactone, and adding rubidium halide and lead halide into the mixture to obtain the product;
(2) X-ray detector for preparing perovskite single crystal
Cleaning the perovskite single crystal generated in the step (1) with ethanol, selecting the upper and lower smooth surfaces, and performing gold electrode evaporation on two sides of the single crystal by using a square electrode template to prepare the perovskite single crystal X-ray detector.
2. Method for producing a perovskite single crystal X-ray detector according to claim 1, characterized in that the added (NH) 2 CH＝NH 2 ) I, rubidium halide, pbI 2 The molar ratio of the lead halide to the lead halide is (0.9-1) to (0-0.1) to (0.8-1) to (0-0.2).
3. Method for producing a perovskite single crystal X-ray detector according to claim 2, characterized in that the added (NH) 2 CH＝NH 2 ) I, rubidium halide, pbI 2 And a lead halide in a molar ratio of 0.95.
4. Method for producing a perovskite single crystal X-ray detector according to claim 2, characterized in that the added (NH) 2 CH＝NH 2 ) I, rubidium halide, pbI 2 And lead halide in a molar ratio of 0.9.
5. Method for producing a perovskite single crystal X-ray detector according to claim 2, characterized in that the added (NH) 2 CH＝NH 2 ) I, rubidium halide, pbI 2 And a molar ratio of lead halide of 0.95.
6. The method for producing a perovskite single crystal X-ray detector as claimed in any one of claims 1 to 5, wherein the perovskite single crystal X-ray detector comprises a perovskite single crystal and electrodes on both upper and lower sides of the single crystal, wherein the perovskite single crystal is (NH) 2 CH＝NH 2 )PbI 3 The molecular formula of the perovskite single crystal growth solution is (NH) prepared by adding rubidium halide and lead halide 2 CH＝NH 2 ) x Rb 1-x Pb(I y Br 1-y ) 3 Wherein 0.9 ≦ x < 1,0.8 ≦ y < 1.
7. The method for producing a perovskite single crystal X-ray detector as claimed in claim 6, wherein the electrode material is gold.
8. The method for preparing a perovskite single crystal X-ray detector as claimed in claim 6, wherein the electrodes are made using a square electrode template with a gold plating layer of 100nm thickness.
9. The method for preparing a perovskite single crystal X-ray detector as claimed in claim 6, wherein said rubidium halide is rubidium iodide or rubidium bromide.
10. The method for producing a perovskite single crystal X-ray detector as claimed in claim 6, wherein the lead halide is lead iodide or lead bromide.
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| CN113046829A (en) * | 2019-12-26 | 2021-06-29 | 四川大学 | Method for inducing halide perovskite single crystal to become impurity intermediate band semiconductor |
| CN111933803A (en) * | 2020-08-20 | 2020-11-13 | 西安电子科技大学 | Nuclear radiation detector based on two-dimensional perovskite single crystal and preparation method thereof |
| CN113823741A (en) * | 2021-08-05 | 2021-12-21 | 中国科学院深圳先进技术研究院 | X-ray active material and preparation method and application thereof |
| CN114380739A (en) * | 2021-12-09 | 2022-04-22 | 山西大学 | Two-dimensional double-layer DJ type perovskite constructed by aromatic amine and preparation method and application thereof |
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